CN112986373A - Ion mobility spectrometry and application thereof - Google Patents
Ion mobility spectrometry and application thereof Download PDFInfo
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- CN112986373A CN112986373A CN201911288763.XA CN201911288763A CN112986373A CN 112986373 A CN112986373 A CN 112986373A CN 201911288763 A CN201911288763 A CN 201911288763A CN 112986373 A CN112986373 A CN 112986373A
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- water vapor
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- ion mobility
- mobility spectrometry
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- 238000001871 ion mobility spectroscopy Methods 0.000 title claims description 34
- 150000002500 ions Chemical class 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 33
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001228 spectrum Methods 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 239000012159 carrier gas Substances 0.000 claims description 39
- 239000007789 gas Substances 0.000 claims description 31
- 238000013508 migration Methods 0.000 claims description 20
- 230000005012 migration Effects 0.000 claims description 20
- -1 polytetrafluoroethylene Polymers 0.000 claims description 17
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 17
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims description 13
- 239000010935 stainless steel Substances 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 238000005485 electric heating Methods 0.000 claims description 8
- 230000005587 bubbling Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims 2
- 239000002184 metal Substances 0.000 claims 1
- 150000002828 nitro derivatives Chemical class 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 6
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 230000002285 radioactive effect Effects 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 20
- 229910052759 nickel Inorganic materials 0.000 description 9
- 229910052743 krypton Inorganic materials 0.000 description 3
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000451 chemical ionisation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/622—Ion mobility spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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- Health & Medical Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Toxicology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
本发明公开了一种离子迁移谱及其应用。本离子迁移谱采用丁酮/水双分子做试剂分子，利用真空紫外灯将丁酮/水转化为水合离子。本离子迁移谱具有非放射性，以水合离子做试剂离子，有助于提高极性化合物的检测灵敏度。离子迁移谱的结构包括：真空紫外灯、离子迁移谱反应区、试剂分子发生装置等。
The invention discloses an ion mobility spectrum and its application. This ion mobility spectrometer uses butanone/water bimolecules as reagent molecules, and uses a vacuum ultraviolet lamp to convert butanone/water into hydrated ions. The ion mobility spectrum is non-radioactive and uses hydrated ions as reagent ions, which helps to improve the detection sensitivity of polar compounds. The structure of ion mobility spectrum includes: vacuum ultraviolet lamp, ion mobility spectrum reaction area, reagent molecule generating device, etc.
Description
Technical Field
The invention belongs to the technical field of ion mobility spectrometry. The ion mobility spectrometry ionization source adopts butanone/water bimolecules as reagent molecules, and converts butanone/water into hydrated ions by using a vacuum ultraviolet lamp. The ion mobility spectrometry ionization source has nonradioactivity, takes hydrated ions as reagent ions, and is beneficial to improving the detection sensitivity of polar compounds.
Technical Field
The hydrated ion is a reagent ion with wider application, has the proton affinity of 696kJ/mol, has higher selectivity, and has non-selectivity for detecting polar compounds, particularly polar inorganic compoundsA great advantage is often achieved. The ionization source capable of generating hydrated ions in the mobility spectrometry at present is mainly radioactive63A Ni ionization source and a corona discharge ionization source. Under the condition of yellow defence [ CN201510890326.0 ], nickel source ion mobility spectrometry is utilized to realize on-line monitoring of ammonia gas by taking hydrated ions as reagent molecules. The radioactivity of the nickel source ionization source limits its wide use in ion mobility spectrometry.
The vacuum ultraviolet ionization source is a soft ionization source, wherein the main photon energy of the krypton lamp is 10.0eV, the ionization energy of water is 12.6eV, and therefore, water cannot be directly ionized by the krypton lamp, and therefore, hydrated ion reagent ions cannot be generated.
Disclosure of Invention
The invention aims to provide a novel ion mobility spectrometry, and an ionization source of the ion mobility spectrometry combines vacuum ultraviolet photoionization and chemical ionization to generate hydrated ionic reagent ions so as to realize effective ionization and detection of polar compounds, particularly polar inorganic compounds.
An ionization source for ion mobility spectrometry comprising: an ion mobility spectrometry reaction zone, a vacuum ultraviolet lamp and a reagent molecule generating device.
The ion migration spectrum comprises a reaction area, a migration area and a signal acquisition and receiving area. The ion migration tube reaction area and the ion migration tube migration area are separated by a grid mesh. A vacuum ultraviolet lamp serving as an ionization source is arranged at the left end of the reaction zone of the ion transfer tube, a carrier gas inlet and a tail gas outlet are arranged on the outer wall surface close to the left side of the reaction zone of the ion transfer tube, a water vapor inlet is arranged on the outer wall surface close to the middle part of the reaction zone of the ion transfer tube, and a sample inlet is arranged on the outer wall surface close to the right side of the reaction zone of the ion transfer tube;
the carrier gas inlet is connected with a carrier gas source through a reagent molecule generating device;
the water vapor inlet is connected with a carrier gas source through a water vapor generating device;
the water vapor generating device is a closed container filled with water, carrier gas of a carrier gas source extends to the position below the water surface in the container through a pipeline, and water vapor is taken out of the container in a bubbling mode and enters the reaction area through a water vapor inlet;
the reagent molecule generator is one sealed container with gas inlet and gas outlet, the carrier gas source is communicated with the gas inlet, the gas outlet is connected via pipeline to the carrier gas inlet, one container with butanone filled in the container is set inside the sealed container, and the volatilized reagent molecule butanone is carried to the reaction area via the carrier gas.
The reaction zone is formed by stacking a stainless steel electrode ring and a polytetrafluoroethylene insulating ring. The thickness of the stainless steel electrode ring is 0.35 cm. The thickness of the polytetrafluoroethylene insulating ring is 1 cm. The vacuum ultraviolet lamp is axially arranged perpendicular to the stainless steel electrode ring and the polytetrafluoroethylene insulating ring, and the center of the vacuum ultraviolet lamp is positioned on the axis of the stainless steel electrode ring and the axis of the polytetrafluoroethylene insulating ring.
A carrier gas inlet and a tail gas outlet are respectively arranged at the positions close to the polytetrafluoroethylene insulation opposite to the vacuum ultraviolet lamp. A water vapor inlet is formed in the polytetrafluoroethylene insulating ring on the right side of the tail gas outlet, and a sample inlet is formed in the polytetrafluoroethylene insulating ring on the right side of the water vapor inlet. The carrier gas enters the ion mobility spectrometry reaction area through the reagent molecule generating device. And water vapor enters the ion mobility spectrometry reaction area through the water vapor inlet. The sample gas enters the ion mobility spectrometry reaction area through the sample inlet. And tail gas is discharged out of the ion mobility spectrometry reaction area through a tail gas outlet.
The inner wall of the reagent molecule generating device is provided with an electric heating device, namely, the inner wall surface of the reagent molecule generating device is provided with an electric heating belt or an electric heating wire and the like, the side wall of the reagent molecule generating device is provided with a thermocouple temperature measuring element, the temperature measuring thermocouple is in signal connection with a temperature controller through a lead, and the electric heating device is connected with an external circuit through the temperature controller.
Reagent molecules butanone and water. The relative humidity of water vapor is 100%
The flow rate of the carrier gas is 50-100ml/min, the flow rate of the water vapor is 100-
The carrier gas and the gas generating water vapor are purified clean air;
the temperature range of the ion transfer tube is between 90 and 150 ℃.
The invention has the advantages that:
the invention provides an ion mobility spectrometry, wherein an ionization source has no radioactivity and can generate hydrated reagent ions with higher signal intensity than a nickel source ionization source, so that the ionization efficiency and the detection sensitivity of a target compound can be improved.
Drawings
FIG. 1 is a schematic view of ion mobility spectrometry. Wherein: 1 is a reaction zone, 2 is a migration zone, 3 is a stainless steel grid, 4 is a signal acquisition and receiving zone, 5 is a carrier gas, 6 is a reagent molecule generation device, 7 is a vacuum ultraviolet lamp, 8 is a tail gas outlet, 9 is a water vapor inlet, 10 is a sample gas inlet, 11 is a floating gas inlet, 12 is a Faraday disc, 13 is an amplifier, 14 is an acquisition card and a computer, 15 is a stainless steel electrode, and 16 and 17 are polytetrafluoroethylene insulating rings.
FIG. 2 is a comparison of signal intensity of hydrated ions generated by a nickel source and a new ionization source;
FIG. 3 is a migration spectrum of 20ppb ammonia measured using a new ionization source
Detailed description of the preferred embodiments
The following examples illustrate the use of the invention without limiting the scope of application described.
An ion mobility spectrometry comprises an ion mobility tube reaction area, an ion mobility tube migration area and an ion mobility tube signal acquisition and receiving area. The ion migration tube reaction area and the ion migration tube migration area are separated by a grid mesh. A vacuum ultraviolet lamp serving as an ionization source is arranged at the left end of the reaction zone of the ion transfer tube, a carrier gas inlet and a tail gas outlet are arranged on the outer wall surface close to the left side of the reaction zone of the ion transfer tube, a water vapor inlet is arranged on the outer wall surface close to the middle part of the reaction zone of the ion transfer tube, and a sample inlet is arranged on the outer wall surface close to the right side of the reaction zone of the ion transfer tube;
the carrier gas inlet is connected with a carrier gas source through a reagent molecule generating device;
the water vapor inlet is connected with a carrier gas source through a water vapor generating device;
the water vapor generating device is a closed container filled with water, carrier gas of a carrier gas source extends to the position below the water surface in the container through a pipeline, and water vapor is taken out of the container in a bubbling mode and enters the reaction area through a water vapor inlet;
the reagent molecule generator is one sealed container with gas inlet and gas outlet, the carrier gas source is communicated with the gas inlet, the gas outlet is connected via pipeline to the carrier gas inlet, one container with butanone filled in the container is set inside the sealed container, and the volatilized reagent molecule butanone is carried to the reaction area via the carrier gas.
Example 1
The performance of the ionization source is inspected, a vacuum ultraviolet lamp is a krypton lamp with 10.0eV, and the ionization source is applied to ion mobility spectrometry. The carrier gas flow rate was 50ml/min, the water vapor flow rate was 260ml/min, and the reaction zone temperature was 150 ℃. As shown in FIG. 2, the signal intensity of the reagent ions obtained from the new ionization source is about 4000mV, which is 4 times that of the nickel source ionization source. The sensitivity of the ionization source is higher than that of the nickel source.
The nickel source adopts radioactivity as ionization source63Ni is used as an ionization source, and a common geometric structure is a cylinder shape in an ion mobility spectrum, and the nickel source ionization source can generate energy of about 17 KeV. In the positive ion mode, the reagent ions generated by the ionization source of the nickel source are hydrated ions. Example 2
The performance of the ion mobility spectrometry described in the present invention was examined. The ion mobility spectrometry is applied to the ion mobility spectrometry, 20ppb ammonia gas is introduced through a sample injection port, and the ion mobility spectrometry of the obtained ammonia gas is shown in figure 3. The ionization source has higher sensitivity for detecting ammonia gas, and the lower limit of detection (LOD) is 0.22 ppb. And the ionization source is carried out under the condition of 100% relative humidity, so that the influence of humidity on ammonia gas detection can be avoided, and the ionization source has very important significance for practical application.
Claims (9)
1. An ion mobility spectrometry, comprising:
the ion migration spectrum comprises a reaction area, a migration area and a signal acquisition and receiving area. The ion migration tube reaction area and the ion migration tube migration area are separated by a grid mesh. A vacuum ultraviolet lamp serving as an ionization source is arranged at the left end of the reaction zone of the ion transfer tube, a carrier gas inlet and a tail gas outlet are arranged on the outer wall surface close to the left side of the reaction zone of the ion transfer tube, a water vapor inlet is arranged on the outer wall surface close to the middle part of the reaction zone of the ion transfer tube, and a sample inlet is arranged on the outer wall surface close to the right side of the reaction zone of the ion transfer tube;
the carrier gas inlet is connected with a carrier gas source through a reagent molecule generating device;
the water vapor inlet is connected with a carrier gas source through a water vapor generating device;
the water vapor generating device is a closed container filled with water, carrier gas of a carrier gas source extends to the position below the water surface in the container through a pipeline, and water vapor is taken out of the container in a bubbling mode and enters the reaction area through a water vapor inlet;
the reagent molecule generator is one sealed container with gas inlet and gas outlet, the carrier gas source is communicated with the gas inlet, the gas outlet is connected via pipeline to the carrier gas inlet, one container with butanone filled in the container is set inside the sealed container, and the volatilized reagent molecule butanone is carried to the reaction area via the carrier gas.
2. The ion mobility spectrometry of claim 1, wherein: the reaction zone is composed of a stainless steel electrode ring
And polytetrafluoroethylene insulating ring
Alternately stacking; stainless steel electrode ring
Is 0.35cm thick, and is made of polytetrafluoroethylene insulating ring
Is 1 cm; optical axis of emergent light of vacuum ultraviolet lamp and stainless steel electrode ring
And polytetrafluoroethylene insulating ring
Coaxially arranged with its optical axis at the stainless steel electrode ring
And polytetrafluoroethylene insulating ring
On the axis of (a).
Migration zone is made of stainless steel electrode ring
And polytetrafluoroethylene insulating ring
Alternately stacking; the thickness of the stainless steel electrode ring is 0.35cm, and the polytetrafluoroethylene insulating ring
Is 0.15 cm.
The migration zone and the reaction zone are isolated by two stainless steel metal grids.
The signal acquisition and receiving area is composed of a Faraday disc
Amplifier with a high-frequency amplifier
Collection card and computer
And (4) forming.
3. The ion mobility spectrometry according to claim 1 or 2, wherein:
the polytetrafluoroethylene insulation close to the vacuum ultraviolet lamp
A carrier gas inlet and a tail gas outlet are respectively arranged at the opposite positions;
a water vapor inlet is arranged on the polytetrafluoroethylene insulating ring on the right side of the tail gas outlet (r), and a sample inlet is arranged on the polytetrafluoroethylene insulating ring on the right side of the water vapor inlet (r); the carrier gas enters into the first ion migration spectrum reaction zone through a reagent molecule generating device; water vapor enters an ion mobility spectrometry reaction area through a water vapor inlet; the sample gas enters into ion migration spectrum reaction zone (I) through sample inlet (R); the tail gas is discharged out of the ion mobility spectrometry reaction area (I) through a tail gas outlet (I).
4. The ion mobility spectrometry of claim 1, wherein: the inner wall of the reagent molecule generating device is provided with an electric heating device, namely, the inner wall surface of the reagent molecule generating device is provided with an electric heating belt and/or an electric heating wire, the side wall inside the reagent molecule generating device is provided with a thermocouple temperature measuring element, the thermocouple temperature measuring element is connected with a temperature controller through a lead by signal, and the electric heating device is connected with an external circuit through the temperature controller.
5. The ion mobility spectrometry of claim 1, wherein: the relative humidity of the gas introduced by the water vapor inlet is 100%.
6. The ion mobility spectrometry of claim 1, wherein: the flow rate of carrier gas at the carrier gas inlet is 50-100ml/min, the flow rate of water vapor at the water vapor inlet is 100-200ml/min, and the sample gas inlet amount is 100-300 ml/min.
7. The ion mobility spectrometry of claim 1, wherein: the carrier gas carrying the reagent molecule butanone and the carrier gas generating the water vapor are purified clean air.
8. The ion mobility spectrometry of claim 1, wherein: the temperature of the reaction zone ranges from 90 ℃ to 150 ℃.
9. Use of the ion mobility spectrometry according to claims 1 to 8, wherein: it can be used for detecting one or more of polar compounds such as ammonia gas, trimethylamine and nitro compounds.
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| CN201911288763.XA CN112986373A (en) | 2019-12-12 | 2019-12-12 | Ion mobility spectrometry and application thereof |
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|---|---|---|---|
| CN201911288763.XA CN112986373A (en) | 2019-12-12 | 2019-12-12 | Ion mobility spectrometry and application thereof |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050109930A1 (en) * | 2003-10-14 | 2005-05-26 | Hill Herbert H.Jr. | Ion mobility spectrometry method and apparatus |
| CN106030299A (en) * | 2013-12-19 | 2016-10-12 | 汉诺威戈特弗里德威廉莱布尼茨大学 | Gas analysis device and method for performing gas analysis |
| CN108088892A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of SF6On-line rapid measurement device and method |
| CN109884158A (en) * | 2017-12-06 | 2019-06-14 | 中国科学院大连化学物理研究所 | A non-radioactive method for online monitoring of ammonia |
| US20190272988A1 (en) * | 2018-03-01 | 2019-09-05 | Shimadzu Corporation | Ion transport device and ion mobility spectrometer |
| CN209356445U (en) * | 2018-11-25 | 2019-09-06 | 中国科学院大连化学物理研究所 | A Sample Injection Structure for Improving the Sensitivity of Ion Mobility Spectrometry |
| CN110431411A (en) * | 2017-01-31 | 2019-11-08 | 史密斯探测-沃特福特有限公司 | Method and apparatus |
| CN110504154A (en) * | 2018-11-25 | 2019-11-26 | 中国科学院大连化学物理研究所 | A highly airtight ion transfer tube |
-
2019
- 2019-12-12 CN CN201911288763.XA patent/CN112986373A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050109930A1 (en) * | 2003-10-14 | 2005-05-26 | Hill Herbert H.Jr. | Ion mobility spectrometry method and apparatus |
| CN106030299A (en) * | 2013-12-19 | 2016-10-12 | 汉诺威戈特弗里德威廉莱布尼茨大学 | Gas analysis device and method for performing gas analysis |
| CN108088892A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of SF6On-line rapid measurement device and method |
| CN110431411A (en) * | 2017-01-31 | 2019-11-08 | 史密斯探测-沃特福特有限公司 | Method and apparatus |
| CN109884158A (en) * | 2017-12-06 | 2019-06-14 | 中国科学院大连化学物理研究所 | A non-radioactive method for online monitoring of ammonia |
| US20190272988A1 (en) * | 2018-03-01 | 2019-09-05 | Shimadzu Corporation | Ion transport device and ion mobility spectrometer |
| CN209356445U (en) * | 2018-11-25 | 2019-09-06 | 中国科学院大连化学物理研究所 | A Sample Injection Structure for Improving the Sensitivity of Ion Mobility Spectrometry |
| CN110504154A (en) * | 2018-11-25 | 2019-11-26 | 中国科学院大连化学物理研究所 | A highly airtight ion transfer tube |
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